#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/75/2017537.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017537
loop_
_publ_author_name
'Becker, Clifford A. L.'
'Black, Robert S.'
'Forbes, Roy P.'
_publ_section_title
;
 Tris(tert-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(I) perchlorate
 dichloromethane disolvate and tris(tert-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(II)
 bis(perchlorate) dichloromethane disolvate: modification of a
 trigonal--bipyramidal structure with change of metal oxidation state
;
_journal_coeditor_code           TR3058
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m40
_journal_page_last               m43
_journal_paper_doi               10.1107/S0108270109054626
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Co (C5 H9 N)3 (C21 H21 O3 P)2] Cl O4, 2(C H2 Cl2)'
_chemical_formula_moiety         'C57 H69 Co N3 O6 P2 +, Cl O4 -, 2(C H2 Cl2)'
_chemical_formula_sum            'C59 H73 Cl5 Co N3 O10 P2'
_chemical_formula_weight         1282.32
_chemical_name_systematic
;Tris(tert-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(I)
perchlorate
 dichloromethane disolvate
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.7568(3)
_cell_length_b                   21.7568(3)
_cell_length_c                   23.3983(6)
_cell_measurement_reflns_used    7171
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.56
_cell_volume                     9591.9(3)
_computing_cell_refinement       'SAINT-NT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-NT (Bruker, 2005)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND
(Brandenburg, 1997)
;
_computing_publication_material
;
WinGX (Farrugia, 1999) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46534
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.8087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4020
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0695P)²+16.3243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.152
_reflns_number_gt                4167
_reflns_number_total             6456
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tr3058.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               2017537
_cod_database_fobs_code          2017537
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.57951(16) 0.28994(16) 0.62264(12) 0.0221(6) Uani d . 1 . .
C C2 0.52705(17) 0.30234(17) 0.64370(14) 0.0275(7) Uani d . 1 . .
H H2 0.5358 0.3295 0.6776 0.033 Uiso calc R 1 . .
C C3 0.46170(18) 0.27565(18) 0.61607(14) 0.0310(7) Uani d . 1 . .
H H3 0.4267 0.2855 0.6304 0.037 Uiso calc R 1 . .
C C4 0.44879(17) 0.23489(17) 0.56771(14) 0.0298(8) Uani d . 1 . .
C C5 0.49963(18) 0.21963(19) 0.54749(15) 0.0334(8) Uani d . 1 . .
H H5 0.4897 0.1899 0.515 0.04 Uiso calc R 1 . .
C C6 0.56455(17) 0.24743(17) 0.57442(13) 0.0280(7) Uani d . 1 . .
H H6 0.5994 0.2374 0.5599 0.034 Uiso calc R 1 . .
O O1 0.38749(13) 0.20628(14) 0.53635(11) 0.0432(7) Uani d . 1 . .
C C7 0.3371(2) 0.2278(2) 0.55046(17) 0.0472(10) Uani d . 1 . .
H H7A 0.3211 0.2142 0.59 0.071 Uiso calc R 1 . .
H H7B 0.2963 0.2046 0.5246 0.071 Uiso calc R 1 . .
H H7C 0.3594 0.2794 0.5465 0.071 Uiso calc R 1 . .
C C8 0.7582(2) 0.3524(2) 0.75 0.0211(9) Uani d S 1 . .
N N1 0.8165(2) 0.3648(2) 0.75 0.0304(9) Uani d S 1 . .
C C9 0.8899(2) 0.3808(3) 0.75 0.0289(10) Uani d S 1 . .
C C10 0.9359(3) 0.4616(3) 0.75 0.0457(14) Uani d S 1 . .
H H10A 0.9188 0.4815 0.7205 0.069 Uiso calc PR 0.5 . .
H H10B 0.9853 0.4751 0.742 0.069 Uiso calc PR 0.5 . .
H H10C 0.9331 0.4801 0.7875 0.069 Uiso calc PR 0.5 . .
C C11 0.9005(2) 0.3484(2) 0.69623(16) 0.0439(10) Uani d . 1 . .
H H11A 0.8695 0.2968 0.6974 0.066 Uiso calc R 1 . .
H H11B 0.9501 0.36 0.6938 0.066 Uiso calc R 1 . .
H H11C 0.8887 0.3676 0.6627 0.066 Uiso calc R 1 . .
P P1 0.6667 0.3333 0.65677(5) 0.0182(3) Uani d S 1 . .
Co Co1 0.6667 0.3333 0.75 0.0175(2) Uani d S 1 . .
C C12 0.06759(15) 0.08358(15) 0.62508(12) 0.0194(6) Uani d . 1 . .
C C13 0.09576(16) 0.08764(17) 0.57080(13) 0.0255(7) Uani d . 1 . .
H H13 0.0804 0.0455 0.5492 0.031 Uiso calc R 1 . .
C C14 0.14572(17) 0.15222(18) 0.54803(13) 0.0279(7) Uani d . 1 . .
H H14 0.1638 0.1543 0.5107 0.033 Uiso calc R 1 . .
C C15 0.16947(17) 0.21403(17) 0.57956(14) 0.0263(7) Uani d . 1 . .
C C16 0.14373(17) 0.21131(17) 0.63387(14) 0.0275(7) Uani d . 1 . .
H H16 0.1605 0.2533 0.656 0.033 Uiso calc R 1 . .
C C17 0.09276(17) 0.14608(16) 0.65579(13) 0.0239(7) Uani d . 1 . .
H H17 0.0746 0.1443 0.693 0.029 Uiso calc R 1 . .
O O2 0.21914(13) 0.27510(12) 0.55329(10) 0.0358(6) Uani d . 1 . .
C C18 0.2456(2) 0.33995(19) 0.58458(17) 0.0448(10) Uani d . 1 . .
H H18A 0.2065 0.3486 0.5931 0.067 Uiso calc R 1 . .
H H18B 0.2815 0.3793 0.5617 0.067 Uiso calc R 1 . .
H H18C 0.267 0.3364 0.6204 0.067 Uiso calc R 1 . .
C C19 -0.0561(2) -0.0970(2) 0.75 0.0200(9) Uani d S 1 . .
N N2 -0.0908(2) -0.1582(2) 0.75 0.0259(8) Uani d S 1 . .
C C20 -0.1388(2) -0.2345(2) 0.75 0.0286(10) Uani d S 1 . .
C C21 -0.2137(3) -0.2461(3) 0.75 0.0411(13) Uani d S 1 . .
H H21A -0.2176 -0.2158 0.7792 0.062 Uiso calc PR 0.5 . .
H H21B -0.2475 -0.296 0.7585 0.062 Uiso calc PR 0.5 . .
H H21C -0.2243 -0.2339 0.7124 0.062 Uiso calc PR 0.5 . .
C C22 -0.1240(2) -0.2645(2) 0.69642(16) 0.0420(9) Uani d . 1 . .
H H22A -0.1313 -0.2424 0.6626 0.063 Uiso calc R 1 . .
H H22B -0.1564 -0.3159 0.695 0.063 Uiso calc R 1 . .
H H22C -0.0749 -0.2546 0.6972 0.063 Uiso calc R 1 . .
P P2 0 0 0.65699(5) 0.0164(3) Uani d S 1 . .
Co Co2 0 0 0.75 0.0161(2) Uani d S 1 . .
C C23 0.37638(16) 0.62157(16) 0.62489(12) 0.0227(7) Uani d . 1 . .
C C24 0.36941(17) 0.56103(17) 0.65066(14) 0.0277(7) Uani d . 1 . .
H H24 0.3424 0.5442 0.6848 0.033 Uiso calc R 1 . .
C C25 0.40075(18) 0.52423(18) 0.62799(14) 0.0297(7) Uani d . 1 . .
H H25 0.3952 0.4828 0.6463 0.036 Uiso calc R 1 . .
C C26 0.44008(18) 0.54894(18) 0.57828(14) 0.0301(8) Uani d . 1 . .
C C27 0.4482(2) 0.6098(2) 0.55204(14) 0.0359(8) Uani d . 1 . .
H H27 0.4755 0.6268 0.5181 0.043 Uiso calc R 1 . .
C C28 0.41658(18) 0.64566(18) 0.57524(14) 0.0300(7) Uani d . 1 . .
H H28 0.4224 0.6873 0.557 0.036 Uiso calc R 1 . .
O O3 0.47361(15) 0.51787(14) 0.55222(10) 0.0417(6) Uani d . 1 . .
C C29 0.4710(2) 0.4579(2) 0.57982(17) 0.0443(10) Uani d . 1 . .
H H29A 0.4892 0.4708 0.6189 0.066 Uiso calc R 1 . .
H H29B 0.5003 0.4431 0.5585 0.066 Uiso calc R 1 . .
H H29C 0.4219 0.4187 0.5809 0.066 Uiso calc R 1 . .
C C30 0.3115(2) 0.7374(2) 0.75 0.0221(9) Uani d S 1 . .
C C31 0.2790(3) 0.8378(3) 0.75 0.0531(10) Uani d S 1 . .
C C32A 0.2012(6) 0.8071(6) 0.75 0.0531(10) Uani d SP 0.544(5) A 2
H H32A 0.181 0.7775 0.7159 0.08 Uiso calc PR 0.272(3) A 2
H H32B 0.1899 0.8454 0.7497 0.08 Uiso calc SPR 0.544(5) A 2
H H32C 0.181 0.778 0.7843 0.08 Uiso calc PR 0.272(3) A 2
C C34A 0.3141(4) 0.8853(4) 0.6974(4) 0.0531(10) Uani d P 0.544(5) A 2
H H34A 0.3651 0.902 0.6977 0.08 Uiso calc PR 0.544(5) A 2
H H34B 0.3067 0.9261 0.6987 0.08 Uiso calc PR 0.544(5) A 2
H H34C 0.2928 0.858 0.6625 0.08 Uiso calc PR 0.544(5) A 2
C C33A 0.2323(5) 0.8255(5) 0.6979(4) 0.0531(10) Uani d P 0.456(5) A 1
H H33A 0.2602 0.8333 0.6631 0.08 Uiso calc PR 0.456(5) A 1
H H33B 0.2141 0.8586 0.6988 0.08 Uiso calc PR 0.456(5) A 1
H H33C 0.1924 0.7767 0.6984 0.08 Uiso calc PR 0.456(5) A 1
C C32B 0.3453(7) 0.9029(7) 0.75 0.0531(10) Uani d SP 0.456(5) A 1
H H32D 0.3714 0.9062 0.7149 0.08 Uiso calc PR 0.228(3) A 1
H H32E 0.3733 0.9043 0.7833 0.08 Uiso calc PR 0.228(3) A 1
H H32F 0.3365 0.9429 0.7518 0.08 Uiso calc SPR 0.456(5) A 1
N N3 0.2961(2) 0.7814(2) 0.75 0.0307(9) Uani d S 1 A .
P P3 0.3333 0.6667 0.65694(5) 0.0186(3) Uani d S 1 . .
Co Co3 0.3333 0.6667 0.75 0.0178(2) Uani d S 1 . .
C C35 0.2752(2) 0.3176(2) 0.42498(17) 0.0466(10) Uani d . 1 . .
H H35A 0.2622 0.3383 0.3927 0.056 Uiso calc R 1 . .
H H35B 0.246 0.3151 0.4583 0.056 Uiso calc R 1 . .
Cl Cl2 0.25520(7) 0.23061(6) 0.40648(4) 0.0574(3) Uani d . 1 . .
Cl Cl3 0.36438(6) 0.37316(7) 0.44143(5) 0.0644(3) Uani d . 1 . .
Cl Cl1 0.00736(8) 0.65908(7) 0.75 0.0453(4) Uani d S 1 . .
O O4 0.0645(3) 0.6441(3) 0.75 0.0901(18) Uani d S 1 . .
O O5 0.0351(2) 0.7339(2) 0.75 0.0631(12) Uani d S 1 . .
O O6 -0.0306(3) 0.6302(2) 0.69993(19) 0.1110(17) Uani d . 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C8 Co1 . . 179.7(4) yes
N2 C19 Co2 . . 179.2(4) yes
N3 C30 Co3 . . 178.6(4) yes
C8 N1 C9 . . 179.7(5) yes
C19 N2 C20 . . 175.8(4) yes
C30 N3 C31 . . 178.4(5) yes
C8 Co1 C8 . 3_665 120.0000(10) ?
C8 Co1 C8 . 2_655 120.000(2) yes
C19 Co2 C19 3 . 120.0000(10) yes
C30 Co3 C30 . 2_665 120.0000(10) yes
P1 Co1 P1 10_557 . 180.0000(10) yes
P2 Co2 P2 . 10_557 180 yes
P3 Co3 P3 10_557 . 180 yes
C2 C1 C6 . . 118.4(3) ?
C2 C1 P1 . . 119.1(2) ?
C6 C1 P1 . . 122.4(2) ?
C1 C2 C3 . . 121.3(3) ?
C1 C2 H2 . . 119.3 ?
C3 C2 H2 . . 119.3 ?
C4 C3 C2 . . 119.0(3) ?
C4 C3 H3 . . 120.5 ?
C2 C3 H3 . . 120.5 ?
O1 C4 C3 . . 124.9(3) ?
O1 C4 C5 . . 114.9(3) ?
C3 C4 C5 . . 120.3(3) ?
C6 C5 C4 . . 120.2(3) ?
C6 C5 H5 . . 119.9 ?
C4 C5 H5 . . 119.9 ?
C5 C6 C1 . . 120.7(3) ?
C5 C6 H6 . . 119.7 ?
C1 C6 H6 . . 119.7 ?
C4 O1 C7 . . 117.3(3) ?
O1 C7 H7A . . 109.5 ?
O1 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
O1 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
N1 C9 C11 . . 107.0(3) ?
N1 C9 C11 . 10_557 107.0(3) ?
C11 C9 C11 . 10_557 112.3(4) ?
N1 C9 C10 . . 106.6(4) ?
C11 C9 C10 . . 111.8(3) ?
C11 C9 C10 10_557 . 111.8(3) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C9 C11 H11A . . 109.5 ?
C9 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C9 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C1 P1 C1 2_655 3_665 102.31(12) ?
C1 P1 C1 2_655 . 102.31(12) ?
C1 P1 C1 3_665 . 102.31(12) ?
C1 P1 Co1 2_655 . 115.93(10) ?
C1 P1 Co1 3_665 . 115.93(10) ?
C1 P1 Co1 . . 115.93(10) ?
C8 Co1 C8 3_665 2_655 120.000(2) ?
C8 Co1 P1 . 10_557 90 yes
C8 Co1 P1 3_665 10_557 90 ?
C8 Co1 P1 2_655 10_557 90 ?
C8 Co1 P1 . . 90 ?
C8 Co1 P1 3_665 . 90 ?
C8 Co1 P1 2_655 . 90 ?
C17 C12 C13 . . 117.7(3) ?
C17 C12 P2 . . 119.4(2) ?
C13 C12 P2 . . 122.9(2) ?
C14 C13 C12 . . 120.9(3) ?
C14 C13 H13 . . 119.6 ?
C12 C13 H13 . . 119.6 ?
C13 C14 C15 . . 120.2(3) ?
C13 C14 H14 . . 119.9 ?
C15 C14 H14 . . 119.9 ?
O2 C15 C16 . . 124.2(3) ?
O2 C15 C14 . . 115.6(3) ?
C16 C15 C14 . . 120.2(3) ?
C15 C16 C17 . . 118.9(3) ?
C15 C16 H16 . . 120.5 ?
C17 C16 H16 . . 120.5 ?
C12 C17 C16 . . 122.2(3) ?
C12 C17 H17 . . 118.9 ?
C16 C17 H17 . . 118.9 ?
C15 O2 C18 . . 117.4(3) ?
O2 C18 H18A . . 109.5 ?
O2 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
O2 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
N2 C20 C21 . . 106.8(4) ?
N2 C20 C22 . . 107.7(3) ?
C21 C20 C22 . . 111.6(3) ?
N2 C20 C22 . 10_557 107.7(3) ?
C21 C20 C22 . 10_557 111.6(3) ?
C22 C20 C22 . 10_557 111.0(4) ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C20 C22 H22A . . 109.5 ?
C20 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C20 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C12 P2 C12 2 . 104.51(11) ?
C12 P2 C12 2 3 104.51(11) ?
C12 P2 C12 . 3 104.51(11) ?
C12 P2 Co2 2 . 114.06(9) ?
C12 P2 Co2 . . 114.06(9) ?
C12 P2 Co2 3 . 114.06(9) ?
C19 Co2 C19 3 2 120.0000(10) ?
C19 Co2 C19 . 2 120 ?
C19 Co2 P2 3 . 90 ?
C19 Co2 P2 . . 90 yes
C19 Co2 P2 2 . 90 ?
C19 Co2 P2 3 10_557 90 ?
C19 Co2 P2 . 10_557 90 ?
C19 Co2 P2 2 10_557 90 ?
C24 C23 C28 . . 118.1(3) ?
C24 C23 P3 . . 119.4(2) ?
C28 C23 P3 . . 122.5(2) ?
C23 C24 C25 . . 121.9(3) ?
C23 C24 H24 . . 119 ?
C25 C24 H24 . . 119 ?
C26 C25 C24 . . 118.9(3) ?
C26 C25 H25 . . 120.6 ?
C24 C25 H25 . . 120.6 ?
O3 C26 C25 . . 124.3(3) ?
O3 C26 C27 . . 115.6(3) ?
C25 C26 C27 . . 120.1(3) ?
C28 C27 C26 . . 120.2(3) ?
C28 C27 H27 . . 119.9 ?
C26 C27 H27 . . 119.9 ?
C27 C28 C23 . . 120.8(3) ?
C27 C28 H28 . . 119.6 ?
C23 C28 H28 . . 119.6 ?
C26 O3 C29 . . 117.7(3) ?
O3 C29 H29A . . 109.5 ?
O3 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
O3 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
N3 C31 C32B . . 106.3(7) ?
N3 C31 C32A . . 109.8(6) ?
C32B C31 C32A . . 143.9(8) ?
N3 C31 C33A . 10_557 106.4(4) ?
C32B C31 C33A . 10_557 115.3(5) ?
C32A C31 C33A . 10_557 53.6(4) ?
N3 C31 C33A . . 106.4(4) ?
C32B C31 C33A . . 115.3(5) ?
C32A C31 C33A . . 53.6(4) ?
C33A C31 C33A 10_557 . 106.3(9) ?
N3 C31 C34A . 10_557 108.5(4) ?
C32B C31 C34A . 10_557 54.5(4) ?
C32A C31 C34A . 10_557 112.0(5) ?
C33A C31 C34A 10_557 10_557 62.8(5) ?
C33A C31 C34A . 10_557 145.1(6) ?
N3 C31 C34A . . 108.5(4) ?
C32B C31 C34A . . 54.5(4) ?
C32A C31 C34A . . 112.0(5) ?
C33A C31 C34A 10_557 . 145.1(6) ?
C33A C31 C34A . . 62.8(5) ?
C34A C31 C34A 10_557 . 105.9(7) ?
C31 C32A H32A . . 109.5 ?
C31 C32A H32B . . 109.5 ?
H32A C32A H32B . . 109.5 ?
C31 C32A H32C . . 109.5 ?
H32A C32A H32C . . 109.5 ?
H32B C32A H32C . . 109.5 ?
C31 C34A H34A . . 109.5 ?
C31 C34A H34B . . 109.5 ?
H34A C34A H34B . . 109.5 ?
C31 C34A H34C . . 109.5 ?
H34A C34A H34C . . 109.5 ?
H34B C34A H34C . . 109.5 ?
C31 C33A H33A . . 109.5 ?
C31 C33A H33B . . 109.5 ?
C31 C33A H33C . . 109.5 ?
C31 C32B H32D . . 109.5 ?
C31 C32B H32E . . 109.5 ?
H32D C32B H32E . . 109.5 ?
C31 C32B H32F . . 109.5 ?
H32D C32B H32F . . 109.5 ?
H32E C32B H32F . . 109.5 ?
C23 P3 C23 3_565 2_665 104.24(11) ?
C23 P3 C23 3_565 . 104.24(12) ?
C23 P3 C23 2_665 . 104.24(12) ?
C23 P3 Co3 3_565 . 114.30(10) ?
C23 P3 Co3 2_665 . 114.30(10) ?
C23 P3 Co3 . . 114.30(10) ?
C30 Co3 C30 . 3_565 120.0000(10) ?
C30 Co3 C30 2_665 3_565 120.0000(10) ?
C30 Co3 P3 . 10_557 90 ?
C30 Co3 P3 2_665 10_557 90 ?
C30 Co3 P3 3_565 10_557 90 ?
C30 Co3 P3 . . 90 yes
C30 Co3 P3 2_665 . 90 ?
C30 Co3 P3 3_565 . 90 ?
Cl3 C35 Cl2 . . 112.8(2) ?
Cl3 C35 H35A . . 109 ?
Cl2 C35 H35A . . 109 ?
Cl3 C35 H35B . . 109 ?
Cl2 C35 H35B . . 109 ?
H35A C35 H35B . . 107.8 ?
O6 Cl1 O6 . 10_557 115.0(5) ?
O5 Cl1 O4 . . 109.8(3) yes
O6 Cl1 O4 . . 106.5(2) yes
O6 Cl1 O5 . . 109.4(2) yes
O6 Cl1 O5 10_557 . 109.4(2) ?
O6 Cl1 O4 10_557 . 106.5(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 C8 3_665 1.820(4) yes
Co2 C19 3 1.834(4) yes
Co3 C30 2_665 1.824(5) yes
P1 Co1 . 2.1814(13) yes
P2 Co2 . 2.1762(12) yes
P3 Co3 . 2.1774(13) yes
C8 N1 . 1.157(6) yes
C19 N2 . 1.158(6) yes
C30 N3 . 1.162(6) yes
N1 C9 . 1.455(6) yes
N2 C20 . 1.453(6) yes
N3 C31 . 1.449(7) yes
C1 C2 . 1.388(4) ?
C1 C6 . 1.390(4) ?
C1 P1 . 1.826(3) ?
C2 C3 . 1.397(5) ?
C2 H2 . 0.95 ?
C3 C4 . 1.377(5) ?
C3 H3 . 0.95 ?
C4 O1 . 1.369(4) ?
C4 C5 . 1.387(5) ?
C5 C6 . 1.380(5) ?
C5 H5 . 0.95 ?
C6 H6 . 0.95 ?
O1 C7 . 1.429(5) ?
C7 H7A . 0.98 ?
C7 H7B . 0.98 ?
C7 H7C . 0.98 ?
C8 Co1 . 1.820(4) ?
C9 C11 . 1.515(4) ?
C9 C11 10_557 1.515(4) ?
C9 C10 . 1.527(7) ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
P1 C1 2_655 1.826(3) ?
P1 C1 3_665 1.826(3) ?
Co1 C8 2_655 1.820(4) ?
Co1 P1 10_557 2.1814(13) ?
C12 C17 . 1.386(4) ?
C12 C13 . 1.394(4) ?
C12 P2 . 1.831(3) ?
C13 C14 . 1.383(4) ?
C13 H13 . 0.95 ?
C14 C15 . 1.388(5) ?
C14 H14 . 0.95 ?
C15 O2 . 1.369(4) ?
C15 C16 . 1.378(5) ?
C16 C17 . 1.390(4) ?
C16 H16 . 0.95 ?
C17 H17 . 0.95 ?
O2 C18 . 1.430(4) ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?
C19 Co2 . 1.834(4) ?
C20 C21 . 1.518(7) ?
C20 C22 . 1.521(4) ?
C20 C22 10_557 1.521(4) ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
P2 C12 2 1.831(3) ?
P2 C12 3 1.831(3) ?
Co2 C19 3 1.834(4) ?
Co2 C19 2 1.834(4) ?
Co2 P2 10_557 2.1762(12) ?
C23 C24 . 1.386(4) ?
C23 C28 . 1.389(4) ?
C23 P3 . 1.822(3) ?
C24 C25 . 1.390(4) ?
C24 H24 . 0.95 ?
C25 C26 . 1.384(5) ?
C25 H25 . 0.95 ?
C26 O3 . 1.362(4) ?
C26 C27 . 1.388(5) ?
C27 C28 . 1.384(5) ?
C27 H27 . 0.95 ?
C28 H28 . 0.95 ?
O3 C29 . 1.432(4) ?
C29 H29A . 0.98 ?
C29 H29B . 0.98 ?
C29 H29C . 0.98 ?
C30 Co3 . 1.824(5) ?
C31 C32B . 1.429(15) ?
C31 C32A . 1.478(13) ?
C31 C33A 10_557 1.523(10) ?
C31 C33A . 1.523(10) ?
C31 C34A 10_557 1.541(9) ?
C31 C34A . 1.541(9) ?
C32A H32A . 0.98 ?
C32A H32B . 0.98 ?
C32A H32C . 0.98 ?
C34A H34A . 0.98 ?
C34A H34B . 0.98 ?
C34A H34C . 0.98 ?
C33A H33A . 0.98 ?
C33A H33B . 0.98 ?
C33A H33C . 0.98 ?
C32B H32D . 0.98 ?
C32B H32E . 0.98 ?
C32B H32F . 0.98 ?
P3 C23 3_565 1.822(3) ?
P3 C23 2_665 1.822(3) ?
Co3 C30 3_565 1.824(5) ?
Co3 P3 10_557 2.1774(13) ?
C35 Cl3 . 1.741(4) ?
C35 Cl2 . 1.772(4) ?
C35 H35A . 0.99 ?
C35 H35B . 0.99 ?
Cl1 O6 10_557 1.389(4) ?
Cl1 O4 . 1.434(5) yes
Cl1 O5 . 1.426(4) yes
Cl1 O6 . 1.389(4) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -2.8(5) ?
P1 C1 C2 C3 . . . . 174.2(3) ?
C1 C2 C3 C4 . . . . 1.5(5) ?
C2 C3 C4 O1 . . . . -179.2(3) ?
C2 C3 C4 C5 . . . . 1.2(5) ?
O1 C4 C5 C6 . . . . 177.9(3) ?
C3 C4 C5 C6 . . . . -2.5(5) ?
C4 C5 C6 C1 . . . . 1.2(5) ?
C2 C1 C6 C5 . . . . 1.4(5) ?
P1 C1 C6 C5 . . . . -175.4(3) ?
C3 C4 O1 C7 . . . . 8.5(5) ?
C5 C4 O1 C7 . . . . -171.9(3) ?
C2 C1 P1 C1 . . . 2_655 170.9(2) ?
C6 C1 P1 C1 . . . 2_655 -12.3(3) ?
C2 C1 P1 C1 . . . 3_665 -83.4(3) ?
C6 C1 P1 C1 . . . 3_665 93.4(2) ?
C2 C1 P1 Co1 . . . . 43.7(3) ?
C6 C1 P1 Co1 . . . . -139.5(2) ?
C1 P1 Co1 C8 2_655 . . . 41.50(17) ?
C1 P1 Co1 C8 3_665 . . . -78.50(17) ?
C1 P1 Co1 C8 . . . . 161.50(17) ?
C1 P1 Co1 C8 2_655 . . 3_665 -78.50(17) ?
C1 P1 Co1 C8 3_665 . . 3_665 161.50(17) ?
C1 P1 Co1 C8 . . . 3_665 41.50(17) ?
C1 P1 Co1 C8 2_655 . . 2_655 161.50(17) ?
C1 P1 Co1 C8 3_665 . . 2_655 41.50(17) ?
C1 P1 Co1 C8 . . . 2_655 -78.50(17) ?
C17 C12 C13 C14 . . . . -1.7(5) ?
P2 C12 C13 C14 . . . . 178.7(2) ?
C12 C13 C14 C15 . . . . 1.1(5) ?
C13 C14 C15 O2 . . . . 179.7(3) ?
C13 C14 C15 C16 . . . . 0.4(5) ?
O2 C15 C16 C17 . . . . 179.4(3) ?
C14 C15 C16 C17 . . . . -1.4(5) ?
C13 C12 C17 C16 . . . . 0.7(5) ?
P2 C12 C17 C16 . . . . -179.6(2) ?
C15 C16 C17 C12 . . . . 0.8(5) ?
C16 C15 O2 C18 . . . . -0.1(5) ?
C14 C15 O2 C18 . . . . -179.3(3) ?
C17 C12 P2 C12 . . . 2 99.7(3) ?
C13 C12 P2 C12 . . . 2 -80.6(2) ?
C17 C12 P2 C12 . . . 3 -150.7(3) ?
C13 C12 P2 C12 . . . 3 28.9(3) ?
C17 C12 P2 Co2 . . . . -25.5(3) ?
C13 C12 P2 Co2 . . . . 154.1(2) ?
C12 P2 Co2 C19 2 . . 3 -45.55(16) ?
C12 P2 Co2 C19 . . . 3 74.45(16) ?
C12 P2 Co2 C19 3 . . 3 -165.55(16) ?
C12 P2 Co2 C19 2 . . . 74.45(16) ?
C12 P2 Co2 C19 . . . . -165.55(16) ?
C12 P2 Co2 C19 3 . . . -45.55(16) ?
C12 P2 Co2 C19 2 . . 2 -165.55(16) ?
C12 P2 Co2 C19 . . . 2 -45.55(16) ?
C12 P2 Co2 C19 3 . . 2 74.45(16) ?
C28 C23 C24 C25 . . . . -0.6(5) ?
P3 C23 C24 C25 . . . . 179.7(3) ?
C23 C24 C25 C26 . . . . 0.1(5) ?
C24 C25 C26 O3 . . . . 179.5(3) ?
C24 C25 C26 C27 . . . . 0.4(5) ?
O3 C26 C27 C28 . . . . -179.6(3) ?
C25 C26 C27 C28 . . . . -0.4(6) ?
C26 C27 C28 C23 . . . . -0.1(6) ?
C24 C23 C28 C27 . . . . 0.6(5) ?
P3 C23 C28 C27 . . . . -179.7(3) ?
C25 C26 O3 C29 . . . . -3.5(5) ?
C27 C26 O3 C29 . . . . 175.7(3) ?
C24 C23 P3 C23 . . . 3_565 -88.9(3) ?
C28 C23 P3 C23 . . . 3_565 91.4(2) ?
C24 C23 P3 C23 . . . 2_665 162.1(3) ?
C28 C23 P3 C23 . . . 2_665 -17.6(3) ?
C24 C23 P3 Co3 . . . . 36.6(3) ?
C28 C23 P3 Co3 . . . . -143.1(2) ?
C23 P3 Co3 C30 3_565 . . . -76.20(17) ?
C23 P3 Co3 C30 2_665 . . . 43.80(17) ?
C23 P3 Co3 C30 . . . . 163.80(17) ?
C23 P3 Co3 C30 3_565 . . 2_665 43.80(17) ?
C23 P3 Co3 C30 2_665 . . 2_665 163.80(17) ?
C23 P3 Co3 C30 . . . 2_665 -76.20(17) ?
C23 P3 Co3 C30 3_565 . . 3_565 163.80(17) ?
C23 P3 Co3 C30 2_665 . . 3_565 -76.20(17) ?
C23 P3 Co3 C30 . . . 3_565 43.80(17) ?
